回春育子颗粒质量标准研究  

Quality Standard of Huichunyuzi Granules

作　　者：曹宝帅 薛刚强[2] 颉维民 潘新艳[3] CAO Baoshuai;XUE Gangqiang;XIE Weimin;PAN Xinyan(Hengshui Comprehensive Testing Center,Hengshui,Hebei,China 050024;Shijiazhuang Fourth Hospital,Shijiazhuang,Hebei,China 050011;Department of Performance Assessment&Quality Management,Hebei General Hospital,Shijiazhuang,Hebei,China 050051)

机构地区：[1]河北省衡水市综合检验检测中心,河北衡水050024 [2]河北省石家庄市第四医院,河北石家庄050011 [3]河北省人民医院绩效考核办公室·质量管理控制办公室,河北石家庄050051

出　　处：《中国药业》2022年第1期66-70,共5页China Pharmaceuticals

基　　金：河北省医学科学研究课题计划项目[20130293]。

摘　　要：目的提高回春育子颗粒的质量标准。方法采用薄层色谱(TLC)法对制剂中的当归、熟地黄、川续断和甘草进行定性鉴别;采用高效液相色谱(HPLC)法测定制剂中原儿茶酸、阿魏酸、柚皮苷、淫羊藿苷和五味子醇甲的含量,色谱柱为WatersSymmetryC_(18)柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.4%磷酸水溶液(梯度洗脱),流速为1.0 mL/min,检测波长分别为260 nm(原儿茶酸)、320 nm(阿魏酸)、283 nm(柚皮苷)、270 nm(淫羊藿苷)、250 nm(五味子醇甲),柱温为35℃,进样量为10μL。结果当归、熟地黄、川续断和甘草的TLC图斑点清晰,分离度好,阴性对照无干扰;原儿茶酸、阿魏酸、柚皮苷、淫羊藿苷和五味子醇甲的质量浓度分别在1.10~55.09μg/mL(r=0.9996),0.96~48.36μg/mL(r=0.9981),0.14~7.11μg/mL(r=0.9979),2.83~141.46μg/mL(r=0.9993),1.00~49.97μg/mL(r=0.9986)范围内与峰面积线性关系良好;检测限分别为5.56,9.77,4.95,5.09,5.02 ng/mL,定量限分别为18.53,32.57,16.50,16.97,16.73 ng/mL;精密度、稳定性、重复性试验结果的RSD均小于2.0%(n=6);加样回收率分别为94.50%,92.28%,99.77%,98.54%,99.14%,RSD分别为1.61%,0.75%,1.34%,0.90%,1.01%(n=6)。结论该方法操作简单,结果准确可靠,重复性和稳定性均较好,可用于回春育子颗粒的质量控制。Objective To improve the quality standard of Huichunyuzi Granules.Methods Thin-layer chromatography(TLC)method was used for the qualitative identification of Angelicae Sinensis Radix,Rehmanniae Radix Praeparata,Dipsaci Radix,Glycyrrhizae Radix et Rhizoma.High-performance liquid chromatography(HPLC)method was used for the content determination of protocatechuic acid,ferulic acid,naringin,icariin and schisandrin.The chromatographic column was Waters Symmetry C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was methanol-0.4%phosphoric acid solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelengths were 260 nm(protocatechuic acid),320 nm(ferulic acid),283 nm(naringin),270 nm(icariin)and 250 nm(schisandrin),the column temperature was 35℃,and the injection volume was 10μL.Results The TLC spots of Angelicae Sinensis Radix,Rehmanniae Radix Praeparata,Dipsaci Radix,Glycyrrhizae Radix et Rhizoma were clear with good resolution,and the negative samples had no interference.The linear ranges of protocatechuic acid,ferulic acid,naringin,icariin and schisandrin were 1.10-55.09μg/mL(r=0.9996),0.96-48.36μg/mL(r=0.9981),0.14-7.11μg/mL(r=0.9979),2.83-141.46μg/mL(r=0.9993)and 1.00-49.97μg/mL(r=0.9986),respectively.The limits of detection(LOD)were 5.56,9.77,4.95,5.09 and 5.02 ng/mL,respectively.The limits of quantitation(LOQ)were 18.53,32.57,16.50,16.97 and 16.73 ng/mL,respectively.The RSDs of precision,stability and reproducibility tests were lower than 2.0%(n=6).The average recoveries of protocatechuic acid,ferulic acid,naringin,icariin and schisandrin were 94.50%,92.28%,99.77%,98.54%and 99.14%with RSDs of 1.61%,0.75%,1.34%,0.90%and 1.01%(n=6),respectively.Conclusion The method is simple,accurate,reliable,reproducible and stable,which can be used for the quality control of Huichunyuzi Granules.

关 键 词：回春育子颗粒 质量标准 薄层色谱法 高效液相色谱法 当归 熟地黄 川续断皂苷Ⅳ 甘草 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学]